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Insert the preferred method of power supply into the handle (Figure 4). The battery and AC Power Supply are keyed and only fit into the analyzer one way
Figure 4. AC battery source inserted into pXRF
You can now turn on the gun. Press the power button on the top of the analyzer for a couple of seconds (Figure 5).
Figure 5. pXRF power button outlined in red. pXRF is off.
The button will illuminate green when on, as shown below in Figure 6.
Figure 6. pXRF turned on
The following step is only applicable at this stage if controlling the pXRF through the computer. If choosing to use the pXRF alone move on to 'Discrete Samples'. The pXRF interface users will use the laptop during the 'Export Files' Section later on.
Open the dedicated pXRF laptop and login to the computer with the following:
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To operate the gun and have it correctly write files administrator privileges are needed. If you login with something different, such as 'daq' 'daq', there are no administrator privileges and the gun will not work properly.
Connect the pXRF to the computer via the micro USB cord (Figure 7). Micro USB ports are very fragile so take care when plugging in or removing.
Figure 7. pXRF connected to laptop via micro USB cable. A. micro USB port. B. Laptop usb port
Discrete Samples
- To set up the discrete sample station collect the FlexStand Base and shielded sample chamber (Figure 8).
Figure 8: FlexStand components. A. FlexStand Base B. Sample Chamber
2. Place the back of the analyzer into the indented portion of the FlexStand Base. The analyzer nose will point into the air as in Figure 9. Take note of the two indents in the analyzer nose.
Figure 9. pXRF in FlexStand base. Red arrow indicating two indents on analyzer nose
3. On the Sample chamber there are two pegs and a release handle (Figure 10). The release handle controls the pegs.
Figure 10. Bottom of Sample Chamber. A. Two pegs B. Release handle
4. The two pegs will fit into the two indents on the analyzer nozzle. Orient the sample chamber so the pegs will fit into the holes and lower the chamber over the nose (Figure 11). The pegs will snap in when inserted.
Figure 11. Sample Chamber resting over pXRF nose.
Note: The Olympus DELTA Flex Stand can be set up in a second orientation, with the instrument standing upright. This is not recommended on board, because the samples are more likely to rock with ship's motion and give inconsistent results.
5. When it is time to remove the sample chamber pull the release handle and while holding the handle, lift off the sample chamber (Figure 12)
Figure 12. Release handle being pulled
Section Halves
In preparing for section half analysis, consider the safety requirements of the instrument. Prepare the area carefully, ensure everyone working with or around the instrument understands X-ray safety, and use the lead drape to protect from scattered X-rays. When the pXRF is in contact with a section half, most of the X-ray energy is absorbed by the sediment/rock. The scattered radiation is at a low (but measurable) level, so maintain reasonable distance between the pXRF and the user. Do not place your hands close to the nose of the instrument; keep them on the grip/trigger area or butt of the instrument.
Remember ALARA: keep your exposure As Low As is Reasonably Achievable.
- Set up an aluminum core tray to hold the unwrapped section half (you will wrap it with Ultralene later, but GLAD® Plastic Wrap is thick enough to interfere with measurements. Place the core tray far enough back from the edge of the bench that the pXRF will be several feet away from the operator.
- Put a long ruler next to the aluminum tray to measure the measurement offset.
- Place the docking station to the side of the core tray.
- Collect the rubber lead impregnated shield. When it is time to take a measurement the pXRF will lock in to the mat as shown in Figure 13.
Figure 13. pXRF being lowered into section half shielding. pXRF oriented with indents facing set screws.
Again, please note that it will be necessary to cover the core surface with Ultralene film and GLAD® Plastic Wrap in order to protect the nose of the instrument and the underside of the shield from contamination. See Preparing Section Halves, below.
Important! Do not measure the core section half without covering it with film!
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- Powdered & dried sample
- Scoopula
- XRF sample cups (32 mm Double Open Ended)
- SPEX Ultralene thin film (0.16 mil; 4 µm thick)
- Whatman Filter Paper Circles (32mm) or Parafilm M® film
- Foam plug
Figure 14. Mortar and pestle along with scoopula. XRF Sample Cup components denoted with red arrows A. Open-end Ring B. Cup C. Cap D. Ultralene® film box E. Whatman Filter Paper F. Foam plug inserts
- A XRF Sample cup has three components: cup, ring, and cap. Take a piece of Ultralene® film and stretch it over one end of the cup. Place the open ring over the film and cup and snap it firmly onto the cup. This will create a tight window on one end of the sample cup (Figure 15). Ultralene® is very thin and prone to ripping. Check for rips before and after sample powder is added.
Figure 15. Ultralene® covering of one side of cup
2. Flip this unit upside down and begin to load the sample into the cup. Remember that the discrete sample will be back loaded. A couple centimeters of sample is sufficient. The sample layer cannot be too thin, or X-ray penetration (and the results) will be inconsistent. Make sure the powder is evenly dispersed, maintaining a relatively flat, even surface.
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Your finished product should look like the cup in Figure 16.
Figure 16. Properly filled XRF cup; note the slight bulge of the powder.
Put a sample label onto the cup. Remove excess Ultralene to help the label stick. The discrete sample is now ready for analysis.
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Double-click the Innov-X Delta Advanced PC Software icon on the desktop (Figure 17) to launch the software.
Figure 17. Innov-X software icon.
The initial start-up window will appear (Figure 18, below); click the Import Data Only button. Import Data Only moves only the analytical data from the pXRF to the PC. If the pXRF was just turned on then wait a moment and select 'Close Device App' then continue with 'Import Data Only'. The PC Software will not let you continue on if the Device Application is active.
Figure 18. Innov-X Start-up Screen
Important! Do not click the Import to PC button!
The Import to PC button overwrites the saved method on the PC with the method stored on the pXRF unit. This is likely to be factory settings and not the methods needed for the analysis, so it is a very undesirable action.
Once the Import Data Only button has been clicked, the Start button will become active after a brief pause to sync the instrument with the software. Click Start. The login screen appears (Figure 19). Enter the following information:
- User Name: innovx
- Password: 1776
Figure 19. Login screen. Login button outlined in red
The main measurement window then pops up.
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Note: When using the Flex Stand, it is possible to perform the Cal Check by simply placing a stainless steel disk on the instrument nose and closing the lid of the Flex Stand. An extra stainless steel disk can be found in the pXRF supplies
Figure 20. Performing a Calibration Check. A. CalCheck Button B. Indicator Bar C. Disabled ‘Start’ button
Click the Cal Check button located on the bottom left as shown in Figure 20, arrow A. The instrument will measure the stainless steel disk and check the peaks and their ratios to ensure that it’s getting the expected results. The Start [analytical measurement] button will remain grayed-out and disabled until the pXRFpasses the CalCheck. If the analyzer fails a Cal Check please refer to the ‘CalCheck Fails’ Section in Troubleshooting.
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Parameters that require setting or editing include: mode and measuring time.
Selecting the Mode
Choose either the Geochemical or the Soil Mode; each one has specific scanning parameters, and preferentially scans certain elements. Discuss with scientists which mode is preferred.
Note: Once a mode is selected, it does not have to be re-chosen before each measurement or when the gun is turned on/off.
Click on Mode, located top right in Figure 21 (arrow A). On the left hand panel, you can choose between Geochemistry and Soil modes (Fig. 21, B). Click on each to see the elements scanned and the beam conditions used in each mode.
Figure 21. Mode window. A. 'Mode' tab B. Measuring Mode options
Selecting Measuring Time
Establish the measuring time for each beam. To access this, click the Set Up button at the top of the screen as shown in Figure 22, arrow A, below. On the left hand panel, click Test Condition. This will show the minimum (Beam # Min) and maximum (Beam # Max) time currently set for each beam. Adjust the settings as desired in seconds and click Save.
Figure 22. Innov-X Set Up Screen. A. Set Up tab B. Test Condition button C. Test Time area D. Save button
The behavior of the Test Time settings is as follows. If the minimum time is set to 1 s and the maximum time is set to 30 s (as shown in Fig. 22), the pXRF will scan until it determines that it has a good profile (via manufacturer-defined quality conditions) and stop measuring before it gets to 30 s. However, even if the pXRF has not reached a "good profile," it will stop at the maximum time.
If the user wants to ensure the pXRF measures for the same time on each measurement, set the minimum and maximum time to the same number (e.g., Beam 1 Min = 30, Beam 1 Max = 30). We do not recommend measurement times below 30 seconds, and longer times may be necessary to get good resolution of weak lines.
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In the Analysis Window, click the blue button with the three dots located in the upper left corner as shown by the B arrow in Figure 23.
Figure 23. Analysis screen closeup. Clicking on the blue "…"
The measurement naming window will appear (Figure 24, below).
Figure 24. Test Information window. IODP-defined fields are circled in red (arrow A). B. Save button
This window contains fields to identify the sample. Arrow A in Figure 24 highlights the IODP-defined editable fields, defined as follows:
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The DELTA's user interface starts with the start-up radiation safety and initialization screens (Figure 25). Read the radiation safety notice screen, and then confirm that you are a certified user
Figure 25. Start-up Radiation safety and initialization screens.
System initialization begins immediately after confirmation (Fig. 26). The analyzer launches a test screen using the previously selected mode.
Figure 26. Initialization and test screens.
Performing a Cal Check
Before sample testing can begin, a Cal Check needs to be performed. This will be shown by a "Cal Check Required" message located on the bottom left of the screen. A Cal Check measurement tells the gun to measure the stainless steel disk located in the stand. This is an internal calibration which ensures the gun is measuring properly.
Note: Cal Checks must be performed when the analyzer requests the procedure (once when the program is started, and once after every ten hours of testing). The Start Test button and trigger are disabled until a successful Cal Check is achieved. The Cal Check can be run any time during software operation, except during a test. When the Cal Check is in progress, the X-ray indicator light assembly blinks. This indicates that the X-ray tube is energized.
To perform a manual Cal Check: Place the analyzer it the DELTA docking station. Tap the Cal Check button.
Note: The deadman trigger are overridden when the analyzer is mounted in the docking station. If necessary, unlock the software trigger lock by tapping the Lock button at the top of the screen.
If the "Cal Check – Passed" message appears on the Results screen, the analyzer is ready for sample testing. If the Cal Check refer to the 'CalCheck fails' section in 'Troubleshooting'.
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Tap the Home button 
. You are now in the main measurement window. First set the Mode in which you'd like to measure in. The gun has a Geochemical and Soil Mode. Each one has different scanning parameters which preferentially pick up some elements better than others. The gun will remember the chosen mode and does not have to be chosen each time a new measurement is taken or the Gun is turned off/on.
To access the Modes click on 'Mode' button 
. This directs you to the 'Mode' Screen where you can choose between the Geochemistry and Soil modes (Figure 27). Click on each to see it's corresponding features and select the one best for your analysis.
Figure 27. Mode Screen.
Now that the Mode is set, establish the measuring time for each beam. Each Mode has preset measuring times but these are changeable. To access the Measurement Time, in the Mode Setup screen click on 'Test Condition.'
In the Test Conditions screen, tap the Test/Tools button 
. This brings you to the Test Setup screen (Fig. 28). Enter the Minimum and Maximum time currently set for each beam (Fig. 28). Adjust the settings to your liking and click 'Save'.
Figure 28. Test Setup screen.
Note: If the minimum time is set to 1 and the maximum to 30, if the gun determines it has a good profile in less than 30 seconds it will stop actively measuring. If you want to ensure it measures for the full time, set the minimum and maximum time to the same number. Ex: Minimum 30s and Maximum 30s
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Dress the green Start button located on the bottom left of the screen as shown in Figure 29, below. The measurement can be started in either the Test Information or Analysis window.
Figure 29. Innov-X Start Button
The spectral graph and elemental concentrations will populate after each beam has completed measuring.
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Navigate to the Test screen (Figure 30). Start the test by pulling the trigger or tapping the Start Test button. 
Figure 30. Start and mid-way through an active test.
The results are displayed immediately upon test completion. Tap the Spectral Plot button to view the spectrum results (Figure 31).
Figure 31. Completed test and results. Results shown as both a list and as a spectrum.
Processing Sample Results
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To export a file, click Set Up on the top right corner of the screen. Click Data Management located on the left hand panel as shown in Figure 32, arrow B.
Figure 32. Accessing the Data Management Screen. A. Set Up tab B. Data Management Button
Once the Data Management screen appears, files can then be exported. The results are organized by date in the window on the right hand-panel as shown in Figure 26. Select the date-referenced file you wish to upload. Make sure the Data or Spectra button is selected (designated by the presence of a check mark; in Figure 30, above, the Data button is selected).
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Other file types are possible, but are not our normal procedure; talk to the technician if you need a different file type.
Once you have selected the type and set the file name, make sure the values are correct as shown in Figure 33.
Figure 33. Exporting a file. A. List of all stored files. B. Data or Spectra selection C. Pathway where exported data goes D. Filename E. Export button
In Figure 33, A indicates the date-referenced data files. These can be exported one by one, or multi-selected. (Or, click Select All to highlight and export all of the files, but this will be difficult to sort out.)
Arrow C indicates the destination path. This should always be set to C:\DATA\IN\. Arrow D is the filename; make sure it matches the file format defined above.
Once the data type (we suggest always starting with Data to help prevent mistakes) is selected, the date-referenced results are selected, the path set, and the filename assigned, click Export. Repeat the process for the Spectra file, again making sure the filename is the same as the Data file. The active filetype has the red checkmark.
After the files have been exported the measurements are attached to the file. Multiple exports can be done in the same day; however, the measurements will still be written to the same date file.
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This step is done by the technician.
Open MegaUploadaTron (MUT). If the file(s) are not yet in the DATA > IN; transfer them now. MUT requires two file types per uploaded file: '.csv' and '.spm'. The filenames must be identical for MUT to recognize the two as linked and MUT will not allow an upload unless both files are present.
Check the boxes for the files to be uploaded. The Misc column identifies files that have not been uploaded as shown in Figure 34.
Figure 34. MUT XRF Uploader.
Click Upload in the bottom right of the window. This brings up the pXRF Pre-upload Form as shown below in Figure 35. This form lists all measurements and allows files to be edited. The fields in white are editable: Run Number, Sample Name, TextID, Offset for SHLF, and Comment. Measurements can also be checked or unchecked to upload or not upload to LIMS. Cross check measurements with the log sheets and make edits as necessary.
Figure 35. MUT pXRF Pre-Upload Form. A indicates the selection boxes. B. Editable fields
Keep a close eye out for duplicate lines. It is easy to inadvertently create multiple measurements with the same name, if the Save button isn't pressed when identifying the sample (see Naming the Sample for Measurement, above).
If any changes need to be made to the editable fields or if scientists require a different file type, from the MUT main screen, click Options > Set active analyses… to open the Configure Acitve Analyses window as shown in Figure 36. Follow the prompts in the window and select Handheld X-Ray Fluorescence Analysis to see the configurable options. The option wheel icon will only appear when the analysis type is on the Active uploaders side and is highlighted.
Figure 36. Configure Active Analyses screen (pXRF shown active).
Once the wheel is clicked, the window in Figure 37 appears.
Figure 37. MUT Settings for pXRF Analysis.
These settings determine what MUT is searching for to validate the data before upload. These values are editable, but it is strongly recommended to have a developer assist you with this. If other labels (see Naming the Sample for Measurement, above) are enabled in the Olympus Innov-X software, those columns can be added here. Add the column name to the EditableColumns value exactly as it appears in the Innov-X menu.
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- WARNING: No one but the operator should be allowed to be closer than 3 feet from the pXRF, particularly the beam port. Ignoring this warning could result in unnecessary exposure.
- WARNING: The operator should never defeat the IR sensor in order to bypass this part of the safety circuit. Defeating this safety feature could result in over-exposure of the operator.
- Do not allow anyone other than trained personnel to operate the pXRF.
- Be aware of the direction that the X-rays travel when the red light is blinking and avoid placing any part of your body (e.g., eyes, hands) near the X-ray port to stabilize the instrument during operation.
- Never hold a sample up to the X-ray port for analysis by hand; hold the instrument to the sample.
- Establish a no-access zone at a sufficient distance from the instruments measurement window, which will allow air and distance to attenuate the beam.
- Enclose the beam working area with protective panels (e.g., >3.0 mm stainless steel) if practical.
- Wear an appropriate dosimeter (see the Laboratory Officer for more information on when a dosimeter is called for).
- The operator is responsible for the security of the handheld XRF. When in use, the device should be in the operator's possession at all times (i.e., either in direct sight or a secure area).
- Always store the instrument in a secure location when not in use.
- During transport to and from the set up location, store the instrument in a cool, dry location.
- WARNING: Pregnant women should not use the pXRF or work in proximity to it. See Additional Note, Pregnancy, above, for more information. Radiation exposure can be harmful to an embryo or developing fetus!